Journal of Pharmaceutical Analysis

2014 Vol. 4, No. 1

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REVIEW ARTICLE
ORIGINAL ARTICLE
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REVIEW ARTICLE

Measurement uncertainty in pharmaceutical analysis and its application

Marcus Augusto Lyrio Traple, Alessandro Morais Saviano, Fabiane Lacerda Francisco, Felipe Rebello Louren?on

2014, (1): 1-5.

Abstract(95) PDF(1)

Abstract:
The measurement uncertainty provides complete information about an analytical result. This is very important because several decisions of compliance or non-compliance are based on analytical results in pharmaceutical industries. The aim of this work was to evaluate and discuss the estimation of uncertainty in pharmaceutical analysis. The uncertainty is a useful tool in the assessment of compliance or non-compliance of in-process and final pharmaceutical products as well as in the assessment of pharmaceutical equivalence and stability study of drug products.

ORIGINAL ARTICLE

Metabolic profiling of plasma from cardiac surgical patients concurrently administered with tranexamic acid:DI-SPME-LC-MS analysis

Barbara Bojko, Marcin W?sowicz, Janusz Pawliszyn

2014, (1): 6-13.

Abstract(85) PDF(0)

Abstract:
A metabolic profile of plasma samples from patients undergoing heart surgery with the use of cardiopulmonary bypass (CPB) and concurrent administration of tranexamic acid was determined. Direct immersion solid phase microextraction (DI-SPME), a new sampling and sample preparation tool for metabolomics, was used in this study for the first time to investigate clinical samples. The results showed alteration of diverse compounds involved in different biochemical pathways. The most significant contribution in changes induced by surgery and applied pharmacotherapy was noticed in metabolic profile of lysophospholipids, triacylglycerols, mediators of platelet aggregation, and linoleic acid metabolites. Two cases of individual response to treatment were also reported.

Identification of metabolites of Radix Paeoniae Alba extract in rat bile, plasma and urine by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry

Zheng-Wei Chen, Ling Tong, Shu-Ming Li, Dong-Xiang Li, Ying Zhang, Shui-Ping Zhou, Yong-Hong Zhu, He Sun

2014, (1): 14-25.

Abstract(131) PDF(0)

Abstract:
Ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF/MS) was developed to identify the absorbed parent components and metabolites in rat bile, plasma and urine after oral administration of Radix Paeoniae Alba extract (RPAE). A total of 65 compounds were detected in rat bile, plasma and urine samples, including 11 parent compounds and 54 metabolites. The results indicated that glucuronidation, hydroxylation and methylation were the major metabolic pathways of the components of RPAE. Furthermore, the results of this work demonstrated that UPLC-Q-TOF/MS combined with MetaboLynx? software and mass defect filtering (MDF) could provide unique high throughput capabilities for drug metabolism study, with excellent MS mass accuracy and enhanced MSE data acquisition. With the MSE technique, both precursor and fragment mass spectra can be simultaneously acquired by alternating between high and low collision energy during a single chromatographic run.

Simultaneous quantitation of atorvastatin and its two active metabolites in human plasma by liquid chromatography/(-) electrospray tandem mass spectrometry

Pankaj Partani, S. Manaswita Verma, Sanjay Gurule, Arshad Khuroo, Tausif Monif

2014, (1): 26-36.

Abstract(129) PDF(1)

Abstract:
A sensitive, accurate and selective liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed and validated for the simultaneous quantitation of atorvastatin (AT) and its equipotent hydroxyl metabolites, 2-hydroxy atorvastatin (2-AT) and 4-hydroxy atorvastatin (4-AT), in human plasma. Electrospray ionization (ESI) interface in negative ion mode was selected to improve the selectivity and the sensitivity required for this application. Additionally, a solid phase extraction (SPE) step was performed to reduce any ion-suppression and/or enhancement effects. The separation of all compounds was achieved in less than 6 min using a C18 reverse-phase fused-cores column and a mobile phase, composed of a mixture of 0.005%formic acid in water:acetonitrile:methanol (35:25:40, v/v/v), in isocratic mode at a flow rate of 0.6 mL/min. The method has lower limit of quantitation (LLOQ) of 0.050 ng/mL for all analytes. The method has shown tremendous reproducibility, with intra-and inter-day precision less than 6.6%, and intra- and inter-day accuracy within 74.3% of nominal values, for all analytes, and has proved to be highly reliable for the analysis of clinical samples.

LC-UV/MS quality analytics of paediatric artemether formulations

Kirsten Vandercruyssen, Matthias D’Hondt, Valentijn Vergote, Herwig Jansen, Christian Burvenich, Bart De Spiegeleer

2014, (1): 37-52.

Abstract(141) PDF(0)

Abstract:
A highly selective and stability-indicating HPLC-method, combined with appropriate sample preparation steps, is developed for β-artemether assay and profiling of related impurities, including possible degradants, in a complex powder for oral suspension. Following HPLC conditions allowed the required selectivity: a Prevail organic acid (OA) column (250 mm×4.6 mm, 5μm), flow rate set at 1.5 mL/min combined with a linear gradient (where A ? 25 mM phosphate buffer (pH 2.5), and B ? acetonitrile) from 30% to 75% B in a runtime of 60 min. Quantitative UV-detection was performed at 210 nm. Acetonitrile was applied as extraction solvent for sample preparation. Using acetonitrile-water mixtures as extraction solvent, a compartmental behaviour by a non-solving excipient-bound fraction and an artemether-solubilising free fraction of solvent was demonstrated, making a mobile phase based extraction not a good choice. Method validation showed that the developed HPLC-method is considered to be suitable for its intended regulatory stability-quality characterisation of β-artemether paediatric formulations. Furthermore, LC-MS on references as well as on stability samples was performed allowing identity confirmation of the β-artemether related impurities. MS-fragmentation scheme of β-artemether and its related substances is proposed, explaining the m/z values of the in-source fragments obtained.

Comparative pharmacokinetics of five saponins after intravenous administration of TSFS injection and TSFS injection plus TFFG in rats under different physiological states

Xiao-Ming Liu, Xing Zhao, En-Ze Gao, Yun-Li Zhao, Zheng Liu, Zhi-Guo Yu

2014, (1): 53-62.

Abstract(101) PDF(1)

Abstract:
Sanqi is a popular traditional Chinese medicine and commonly used for promoting blood circulation and removing blood stasis. Notoginsenoside R1, ginsenoside Rg1, Re, Rb1 and Rd are the major active constituents of Sanqi. The purpose of the study was to investigate the pharmacokinetic behavior of the five active constituents from total saponin from Sanqi when it was used in the blood stasis animals or in combination with Gegen. The concentrations of the five active constituents in rat plasma were determined by an ultra-HPLC-ESI-MS/MS method. The main pharmacokinetic parameters were calculated and statistically analyzed using the unpaired student's t-test. It was found that the pharmacokinetic parameters of notoginsenoside R1, ginsenoside Rg1 and Rb1 represented a statistically significant difference (Po0.05) between the normal rats and the blood stasis rats after administration of total saponin from Sanqi (TSFS). And there were statistically significant differences (Po0.05) in the pharmacokinetic parameters of all the five constituents between administration of TSFS alone and combined with total flavonoid from Gegen (TFFG) in blood stasis rats. It suggested that the pharmacokinetic behavior of the active constituents from TSFS could be changed when it was used in blood stasis animals or in combination with TFFG.

Development of a sensitive and rapid method for quantitation of (S)-(-)- and (R)-(t)-metoprolol in human plasma by chiral LC-ESI-MS/MS

Primal Sharma, Pritesh Contractor, Swati Guttikar, Daxesh P. Patel, Pranav S. Shrivastav

2014, (1): 63-79.

Abstract(74) PDF(0)

Abstract:
A selective, sensitive and high throughput liquid chromatography-tandem mass spectro-metry (LC-ESI-MS/MS) method has been developed for separation and quantification of metoprolol enantiomers on a chiral Lux Amylose-2 (250 mm×4.6 mm, 5 mm) column. Solid phase extraction of (S)-(-)- and (R)-(t)-metoprolol and rac-metoprolol-d6 as an internal standard (IS) was achieved on Lichrosep DVB HL cartridges employing 200 mL human plasma. Both the analytes were chromatographically separated with a resolution factor of 2.24 using 15 mM ammonium acetate in water, pH 5.0 and 0.1% (v/v) diethyl amine in acetonitrile (50:50, v/v) as the mobile phase within 7.0 min. The precursor-product ion transitions for the enantiomers and IS were monitored in the multiple reaction monitoring and positive ionization mode. The method was validated over the concentration range of 0.500-500 ng/mL for both the enantiomers. Matrix effect was assessed by post-column analyte infusion experiment and the mean extraction recovery was greater than 94.0% for both the enantiomers at all quality control levels. The stability of analytes was evaluated in plasma and whole blood under different storage conditions. The method was successfully applied to a clinical study in 14 healthy volunteers after oral administration of 200 mg metoprolol tablet under fasting conditions. The assay reproducibility is shown by reanalysis of 68 incurred samples. The suitability of the developed method was assessed in comparison with different chromatographic methods developed for stereoselective analysis of metoprolol in biological matrices.

INFORMATION

Application of analytical instruments in pharmaceutical analysis

2014, (1): 80-81.

Abstract(115) PDF(1)

Abstract: